CN117059398A - Preparation method of low-loss X9R type leadless ceramic capacitor material - Google Patents
Preparation method of low-loss X9R type leadless ceramic capacitor material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 37
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims description 35
- 238000000498 ball milling Methods 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 15
- 239000003292 glue Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 5
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 20
- 239000003990 capacitor Substances 0.000 description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 230000005684 electric field Effects 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 239000004677 Nylon Substances 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002998 adhesive polymer Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000009475 tablet pressing Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
- H01G13/04—Drying; Impregnating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1254—Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Ceramic Capacitors (AREA)
Abstract
The invention discloses a low-loss X9R type leadless ceramic capacitor material and a preparation method thereof, belonging to the technical field of dielectric energy storage ceramic materials, and comprising a ceramic material with a nominal chemical formula (Ba) 0.85‑ x1.275 La x0.85 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 ‑y wt.%MnO 2 The low-loss X9R type leadless ceramic capacitor material is obtained by five steps, the preparation process is simpler, the cost is greatly reduced, the energy storage performance is excellent, and the energy storage density can reach 3.70J/cm 3 And the temperature stability and the frequency stability are good, the EIAX9R standard is met, harmful components such as lead and the like are not contained, the environment is protected, and the industrial prospect is good.
Description
Technical Field
The invention mainly relates to the technical field of dielectric energy storage ceramic materials, in particular to a preparation method of a low-loss X9R type leadless ceramic capacitor material.
Background
Ceramic capacitors are also called as ceramic dielectric capacitors or monolithic capacitors, and ceramic dielectric capacitors are capacitors with ceramic dielectric materials, and can be classified into low-frequency ceramic capacitors and high-frequency ceramic capacitors according to different ceramic materials, and can be classified into wafer-shaped capacitors, tubular capacitors, rectangular capacitors, chip capacitors, penetrating capacitors and the like according to structural forms.
The ceramic energy storage capacitor has the advantages of high discharge power, high utilization efficiency, large energy storage density rising space, high charge and discharge speed, cyclic aging resistance, suitability for extreme environments such as high temperature and high pressure, stable performance and the like, is becoming an energy storage element in pulse power equipment gradually and being widely used, but has large loss, low energy storage and higher cost, and part of materials in the ceramic capacitor contain harmful components such as lead and the like, can cause certain harm to the environment, is not environment-friendly and does not accord with the concept of environmental protection in China.
Therefore, the development of the high-temperature high-energy-storage density dielectric material with lead-free, high dielectric constant, high breakdown field strength and low dielectric loss has very important effect on the development of the fields of modern electronic energy systems, such as national defense of hybrid electric vehicles, electromagnetic track gun weapons and the like, modern industry and the like.
Barium titanate (BaTiO) 3 BT) is a typical ferroelectric material, and has the characteristics of large dielectric constant, low dielectric loss, curie temperature of about 120 ℃ and the like, and a large number of researches prove that BiMeO with lower tolerance factor is adopted 3 (Me represents a complex trivalent cation) as an additive to broaden BaTiO 3 The high temperature stability range of the ceramic and the relatively high W are obtained rec And η values are one possible strategy [ document 1: xuewei Liang, et al Journal of Materials Science: materials in Electronics 32 (3), 2021:3377-90. It is reported that doping of trace rare earth elements can increase breakdown field strength of dielectric materials, further improving energy storage performance [ document 2: qinghuan Huang, et al, ceramics International (12), 2022:17359-68. In addition, additional studies have shown that Mn incorporation can promote defective dipole formation, withEffectively reduces carrier migration and improves the reliability of the ceramic, on the other hand, the doping of Mn can also effectively reduce Ti 4+ To suppress the deterioration of ferroelectricity, reduce leakage current, and further improve the stability of the capacitor [ document 3: wei Peng, et al Ceramics International 47 (20), 2021:29191-96).
Disclosure of Invention
The technical scheme of the invention aims at the technical problem that the prior art is too single, provides a solution which is obviously different from the prior art, and particularly mainly provides a preparation method of a low-loss X9R type leadless ceramic capacitor material, which is used for solving the technical problems that the existing ceramic energy storage capacitor provided in the background art is low in dielectric constant, high in loss and incapable of being well adapted to the application environment of high temperature and high energy storage.
The technical scheme adopted for solving the technical problems is as follows:
a low-loss X9R type leadless ceramic capacitor material comprises a ceramic material with a nominal chemical formula of (Ba 0.85- 1.275x La 0.85x Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -y wt.％MnO 2 And x in the chemical formula is an atomic ratio of 0.00-0.05, and y in the chemical formula is a mass fraction of 0.00-0.30.
The invention also provides a preparation method of the low-loss X9R type leadless ceramic capacitor material, which comprises the following specific steps:
step 1: in BaCO 3 ，TiO 2 ，Bi 2 O 3 ，MgO，WO 3 ，La 2 O 3 And MnO 2 As a raw material, according to (Ba 0.85- 1.275x La 0.85x Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -ywt.％MnO 2 (x is more than or equal to 0.00 and less than or equal to 0.05,0.00 and y is more than or equal to 0.30, wherein x is an atomic ratio, y is a mass fraction), weighing and proportioning, and then taking absolute ethyl alcohol as a ball milling medium, and carrying out ball milling and mixing uniformly and then drying;
step 2: calcining the dried mixed powder prepared in the step 1 at 800-900 ℃ for 2-3 hours to prepare pre-calcined ceramic powder;
step 3: crushing the pre-sintered ceramic powder prepared in the step 2, and then taking absolute ethyl alcohol as a ball milling medium, performing ball milling and mixing uniformly in a ball milling tank, drying and grinding into micron-sized powder;
step 4: adding 5wt.% of PVA binder into the powder prepared in the step 3, granulating, tabletting and discharging glue to obtain a ceramic block blank;
step 5: sintering the ceramic green body at 1150-1250 ℃ for 2-5 h to obtain the corresponding low-loss X9R type leadless ceramic capacitor material.
Preferably, the purity of all raw materials in the step 1 is more than or equal to 99%.
Preferably, the ball milling time in the step 1 is 6-12 h, the drying temperature is 70-100 ℃, and the drying time is 24-48 h.
Preferably, the ball milling time in the step 3 is 6-12 h, the drying temperature is 70-100 ℃, and the drying time is 24-48 h.
Preferably, the diameter of the tablet pressing die in the step 4 is 10mm-15mm, the pressure is 1MPa-2MPa, and the pressure maintaining time is 15s-45s.
Preferably, the glue discharging temperature in the step 4 is 550-650 ℃ and the glue discharging time is 1.5-2.5 h.
Preferably, in the step 4, the mass ratio of the powder prepared in the step 3 to the PVA adhesive is 10:1.
Compared with the prior art, the invention has the beneficial effects that:
the sample preparation of the invention adopts the traditional solid-phase sintering method, does not need special sintering process (such as hot-press sintering, cold sintering, two-step sintering (TSS) adhesive polymer process (VPP) and the like), thus does not need special equipment to provide high pressure, high temperature or electric field, can be sintered by a common muffle furnace, has simple preparation method and low process cost, and adopts BaCO as raw materials 3 ，TiO 2 The material is mainly modified by doping a small amount of other oxides, the raw materials are simple and easy to obtain, the price is low, and in addition, the material does not contain harmful components such as lead, is nontoxic and harmless, is environment-friendly and has strong practicability;
the sample of the invention has the advantages of high dielectric constant, high breakdown field strength, low dielectric loss and the like, and the total energy storage density (W) and the recoverable energy storage density (W) of the dielectric ceramic material rec ) And the energy storage efficiency (η) can be calculated from the following three formulas:
wherein: p (P) max For maximum polarization intensity, P r E is the strength of the external electric field;
the high dielectric constant, high breakdown field strength and low loss are favorable for obtaining higher polarization and fine P-E ring (electric hysteresis loop), thereby obtaining better energy storage density and higher efficiency, the saturation polarization value and the breakdown electric field are in negative correlation, the higher dielectric constant can ensure to obtain high saturation polarization, the improvement of the breakdown electric field is favorable for further improving the energy storage density, the low loss means low energy loss, the high energy storage density can be obtained and the high efficiency can be maintained, and the energy storage density of the sample in the first embodiment of the invention can reach 3.70J/cm 3 The invention has excellent energy storage performance, and simultaneously has excellent temperature stability and frequency stability, accords with EIAX9R standard, and has good industrialization prospect.
The invention will be explained in detail below with reference to the drawings and specific embodiments.
Drawings
FIG. 1 shows the structure of the present invention (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.10wt.％MnO 2 (i.e. x=0.02,y=0.10), a schematic diagram of the law of the dielectric constant and the loss along with the temperature change of the low-loss X9R type leadless ceramic capacitor material under different frequency conditions;
FIG. 2 shows the structure of the present invention (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.10wt.％MnO 2 A schematic diagram of a law of change rate of dielectric constant of the low-loss X9R type leadless ceramic capacitor material under different frequencies along with temperature change;
FIG. 3 shows the structure of the present invention (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.10wt.％MnO 2 An X-ray diffraction pattern of the low-loss X9R type leadless ceramic capacitor material;
FIG. 4 shows the structure of the present invention (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.10wt.％MnO 2 Microscopic topography of the low-loss X9R type leadless ceramic capacitor material;
FIG. 5 shows the structure of the present invention (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.10wt.％MnO 2 Sample plot of low loss X9R lead free ceramic capacitor material.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will be rendered by reference to the appended drawings, in which several embodiments of the invention are illustrated, but which may be embodied in different forms and are not limited to the embodiments described herein, which are, on the contrary, provided to provide a more thorough and complete disclosure of the invention.
It will be understood that when an element is referred to as being "mounted" on another element, it can be directly on the other element or intervening elements may be present, and when an element is referred to as being "connected" to the other element, it may be directly connected to the other element or intervening elements may also be present, the terms "vertical", "horizontal", "left", "right" and the like are used herein for the purpose of illustration only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly connected to one of ordinary skill in the art to which this invention belongs, and the knowledge of terms used in the description of this invention herein for the purpose of describing particular embodiments is not intended to limit the invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In the first embodiment, please refer to fig. 1-5, the present invention adopts a solid phase reaction method to prepare the low-loss X9R type leadless ceramic capacitor material.
Low-loss X9R type leadless ceramic capacitor material (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.10wt.％MnO 2 The preparation method of (i.e. x=0.02, y=0.10) comprises the following specific steps:
step 1: in BaCO 3 ，TiO 2 ，Bi 2 O 3 ，MgO，WO 3 ，La 2 O 3 And MnO 2 The raw materials are weighed according to the chemical proportion, the ingredients are put into a ball milling tank, zirconia balls and a nylon tank are selected, the mixing ball milling time is 10 hours, the rotating speed is 300 revolutions per minute, and the ball milling medium is absolute ethyl alcohol. And (5) placing the mixture obtained after ball milling in a 90 ℃ oven for drying for 24 hours.
Step 2: and (3) heating the obtained baked powder to 800 ℃ at a heating rate of 5 ℃/min, and calcining for 2 hours to obtain the presintered ceramic powder.
Step 3: the prepared presintered powder is crushed, ball-milled for 10 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixed, dried for 24 hours at 90 ℃, and ground into micron-sized powder.
Step 4: 10g of the prepared powder is added with 1mL of 5wt.% PVA binder, and after being fully ground and uniformly mixed, 0.3g of the powder is put into a die with the diameter of 10mm, the pressure is maintained for 30s under the pressure of 1MPa, and the taken out circular ceramic block is subjected to glue discharging for 2h at the temperature of 600 ℃ to prepare a ceramic block blank.
Step 5: sintering the ceramic block blank after glue discharge at 1225 ℃ for 3 hours to obtain a corresponding ceramic block, namely the corresponding low-loss X9R type lead-free ceramic capacitor material.
Embodiment two:
low-loss X9R type leadless ceramic capacitor material (Ba 0.83725 La 0.0085 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 The preparation method of (i.e. x=0.01, y=0.00) comprises the following specific steps:
step 1: in BaCO 3 ，TiO 2 ，Bi 2 O 3 ，MgO，WO 3 ，La 2 O 3 And MnO 2 The raw materials are weighed according to the chemical proportion, the ingredients are put into a ball milling tank, zirconia balls and a nylon tank are selected, the mixing ball milling time is 6 hours, the rotating speed is 300 revolutions per minute, and the ball milling medium is absolute ethyl alcohol. And (5) placing the mixture obtained after ball milling in a 70 ℃ oven for drying for 48 hours.
Step 2: and (3) heating the obtained baked powder to 850 ℃ at a heating rate of 5 ℃/min, and calcining for 2 hours to obtain the presintered ceramic powder.
Step 3: the prepared presintered powder is crushed, ball-milled for 6 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixed, dried for 48 hours at 70 ℃, and ground into micron-sized powder.
Step 4: 10g of the prepared powder is added with 1mL of 5wt.% PVA binder, and after being fully ground and uniformly mixed, 0.3g of the powder is put into a die with the diameter of 10mm, the pressure is maintained for 25s under the pressure of 1.5MPa, and the taken out circular ceramic block is subjected to glue discharging for 2h at the temperature of 650 ℃ to prepare a ceramic block blank.
Step 5: sintering the ceramic block blank after glue discharge at 1250 ℃ for 3 hours to obtain a corresponding ceramic block, namely the corresponding low-loss X9R type lead-free ceramic capacitor material.
Embodiment III:
low-loss X9R type leadless ceramic capacitor material (Ba 0.8245 La 0.017 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -0.30wt.％MnO 2 The preparation method of (i.e. x=0.02, y=0.30) comprises the following specific steps:
step 1: in BaCO 3 ，TiO 2 ，Bi 2 O 3 ，MgO，WO 3 ，La 2 O 3 And MnO 2 The raw materials are weighed according to the chemical proportion, the ingredients are put into a ball milling tank, zirconia balls and a nylon tank are selected, the mixing ball milling time is 12 hours, the rotating speed is 300 revolutions per minute, and the ball milling medium is absolute ethyl alcohol. And (5) placing the mixture obtained after ball milling in a 100 ℃ oven for drying for 24 hours.
Step 2: and (3) heating the obtained baked powder to 800 ℃ at a heating rate of 5 ℃/min, and calcining for 3 hours to obtain the pre-sintered ceramic powder.
Step 3: the prepared presintered powder is crushed, ball-milled for 12 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixed, dried for 24 hours at 100 ℃, and ground into micron-sized powder.
Step 4: 10g of the prepared powder is added with 1mL of 5wt.% PVA binder, and after being fully ground and uniformly mixed, 0.3g of the powder is put into a die with the diameter of 10mm, the pressure is maintained for 15s under the pressure of 2MPa, and the taken out circular ceramic block is subjected to glue discharging for 2.5 hours at the temperature of 600 ℃ to prepare a ceramic block blank.
Step 5: sintering the ceramic block blank after the glue discharge at 1150 ℃ for 2 hours to obtain a corresponding ceramic block, namely the corresponding low-loss X9R type lead-free ceramic capacitor material.
The dielectric constant and the loss of the barium titanate-based ceramic material prepared in the first embodiment are tested under different frequencies and room temperature conditions, the test results are shown in the attached figure 1, the figure 2 is a rule chart of the dielectric constant change rate of the low-loss X9R ceramic material under different frequencies along with the temperature change, the figure 3 is an XRD chart of the first embodiment sample, which shows that the prepared ceramic sample has a single perovskite structure and no impurity phase, the figure 4 is a surface micro-morphology chart (scanning electron microscope photo) of the first embodiment sample, which shows that the prepared ceramic sample has fine crystal grains and uniform size, and the figure 5 is a physical chart of the first embodiment sample, which is obvious from the figure 2, the prepared dielectric ceramic material has high temperature stability (-55 ℃ -200 ℃) and meets the industry standard (-15% < 15%) of the X9R ceramic capacitor, and has strong practicability and is expected to realize application in the electronic ceramic market.
While the invention has been described above with reference to the accompanying drawings, it will be apparent that the invention is not limited to the embodiments described above, but is intended to be within the scope of the invention, as long as such insubstantial modifications are made by the method concepts and technical solutions of the invention, or the concepts and technical solutions of the invention are applied directly to other occasions without any modifications.
Claims (8)
1. A low-loss X9R type leadless ceramic capacitor material is characterized by comprising a ceramic material with a nominal chemical formula of (Ba 0.85- x1.5 La x Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 - y wt.% MnO 2 And of the formulaxThe atomic ratio is less than or equal to 0.00xLess than or equal to 0.0, in the chemical formulayThe mass fraction is 0.00-0y ≤ 0.30。
2. The preparation method of the low-loss X9R type leadless ceramic capacitor material is characterized by comprising the following specific steps:
step 1: in BaCO 3 ，TiO 2 ，Bi 2 O 3 ，MgO，WO 3 ，La 2 O 3 And MnO 2 As a raw material, according to (Ba 0.85- x1.275 La x0.85 Bi 0.15 )(Mg 0.1125 W 0.0375 Ti 0.85 )O 3 -y wt.%MnO 2 （0.00≤x≤0.05，0.00≤yWeighing and proportioning the materials in a chemical proportion of less than or equal to 0.30), taking absolute ethyl alcohol as a ball milling medium, and drying after ball milling and mixing uniformly;
step 2: calcining the dried mixed powder prepared in the step 1 at 800-900 ℃ for 2-3 hours to prepare pre-calcined ceramic powder;
step 3: crushing the pre-sintered ceramic powder prepared in the step 2, and then taking absolute ethyl alcohol as a ball milling medium, performing ball milling and mixing uniformly in a ball milling tank, drying and grinding into micron-sized powder;
step 4: adding 5wt.% of PVA binder into the powder prepared in the step 3, granulating, tabletting and discharging glue to obtain a ceramic block blank;
step 5: sintering the ceramic green body prepared in the step 4 for 2-5 hours at 1150-1250 ℃ to obtain the corresponding low-loss X9R type leadless ceramic capacitor material.
3. The method for preparing the low-loss X9R lead-free ceramic capacitor material according to claim 2, wherein the purity of all raw materials in the step 1 is more than or equal to 99%.
4. The method for preparing the low-loss X9R lead-free ceramic capacitor material according to claim 2, wherein the ball milling time in the step 1 is 6-12 h, the drying temperature is 70-100 ℃, and the drying time is 24-48 h.
5. The method for preparing the low-loss X9R lead-free ceramic capacitor material according to claim 2, wherein the ball milling time in the step 3 is 6-12 h, the drying temperature is 70-100 ℃, and the drying time is 24-48 h.
6. The method for preparing a low-loss X9R lead-free ceramic capacitor material according to claim 2, wherein the diameter of the die for pressing in the step 4 is 10mm-15mm, the pressure is 1-2 MPa, and the dwell time is 15s-45s.
7. The method for preparing the low-loss X9R type leadless ceramic capacitor material according to claim 2, wherein the glue discharging temperature in the step 4 is 550-650 ℃, and the glue discharging time is 1.5-2.5 h.
8. The method for preparing the low-loss X9R lead-free ceramic capacitor material according to claim 2, wherein in the step 4, the mass ratio of the powder prepared in the step 3 to the PVA binder is 10:1.
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| CN202311003767.5A CN117059398A (en) | 2023-08-10 | 2023-08-10 | Preparation method of low-loss X9R type leadless ceramic capacitor material |
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| CN202311003767.5A Pending CN117059398A (en) | 2023-08-10 | 2023-08-10 | Preparation method of low-loss X9R type leadless ceramic capacitor material |
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